Process of making chloropicrin



UNITED STATES IOWA, ASSIGNOR T0 D. BAKER, SECRETARY OF WAR, TRUSTEE.

OBLAND R. SWEENEY, OF AIVIES,

- Examiner ra'rlal'ar OFFICE.

PROCESS OF MAKING CHLOROPICRIN.

No Drawing.

(FILED UNDER THE ACT OF MARCH 3, 1883, 22 STAT. L, 625.)

T 0 all w 710m it may concern Be it known that I, ORLAND R. SWEENEY, a citizen ofthe United- States, residing in Ames, Iowa, have invented an Improvement in Processes of Making chloropicrin, of which the following is a specification.

The invention described herein may be used by the Government, or any of its officers or employees, in prosecution of work for the Government, or by any other person in the United States, without payment of any royalty thereon.

This invention relates to a process for producing chloropicrin, andhas among its objects the provision of a method whereby the reactions involved in the process are adequately controlled and whereby a maximum yield of chloropicrin may be obtained.

A furtherobject of this invention is the provision of a process whereby the containers for the materials entering into the reaction are protected from destructive solvent action by some of said ingredients.

In carrying out my process I employ a chlorine yielding material such as bleaching powder sodium hypochlorite, liquid bleach or chlorine gas, and these substances may be suspended or otherwise dispersed in water or any suitable medium. A suspenslon or other suitable dispersion of picric acid in water or other convenient medium is also pre and. I have found that in working wit containers of iron the destructive solvent action of the picric acid on the container is very great and detrimental to successful operation of the process. To overcome this effect of the picric acid on the iron, I provide a protective agent such as lime, soda-ash, lime-stone, dolomite or other alkaline substance.

In carrying out this process, the dispersions of the chlorine yielding materiara d thatof the'picric acid and" protective ageiit are preferably thrown against each" other with force'insuch a manner as to thoroughly mix them'f"This "may be accomplished by the same time the reaction is controlled so and picric acid are separately suspended in water, enough lime or other alkali being added" to the suspension of picric acid to keep it alkaline at all times and to prevent the latter from attacking the vessel containlng the picric acid and the iron pipes through which this suspension of picric acid is later conducted. A convenient charge consist-s of about 4000 lbs. of bleaching powder, 400 lbs. of picric acid to 2,000 gals. of water. The substances begin to react just as soon as they are brought together and the chloropicrin is recovered by steam distillation. T oprevent the still from foaming over, a water spray is injected into the still when the formation of foam becomes marked. The distillation with steam is continued until all chloropicrin is removed from the still.

My process will yield from 1,2 to 2.1 pounds chloropicrin per pound of picric acid.

I prefer to have most of the materials suspended in water in the form of sludges rather than as solutions because of the greater facility in preparing such, and because a greater yield of chloropicrin results. However, it is to be understood that this process is not limited to the use of sludges but contemplates the employment of materials in other dispersed forms, such as solutions or emulsions, or combinations of various dispersed forms of the materials.

WVhile the process as disclosed herein is directed to the manufacture of chloropicrin, it is to be understood that applicant does not intend that his invention be limited to the process of making this specific material, as other substances such as brompicrin can be made by this process by the substitution of suitable materials for the ones herein disclosed.

The present invention is not limited to the specific details set forth in the foregoing examples which should be construed as illustrative and not by way of limitation, and in view of the numerous modifications which from the spirit and scope of this invention,

it is desired that only such limitations be imposed as are indicated in the appended claims.

I claim as my invention:

1. In a process of making chloropicrin, bringing together a dispersion in a water comprising medium of a chlorine yielding material and a dispersion in a water comprising medium of picric acid.

2. In a process of making chloropicrin, bringing together a dispersion in a water comprising medium of a chlorine yielding material and a suspension in a water comprising medium of picric acid.

3. In a process of making chloropicrin, bringing together a dispersion in a water comprising medium of a. chlorine yielding material and dispersions in a water comprising medium of picric acid and of an agent for neutralizing the dissolved portion of the picric acid.

42. In a process of making chloropicrin, bringing together a dispersion in a Water comprising medium of a chlorine yielding material and dispel-sons in a water comprising medium of picric acid and of an alkali.

5. In a process of making chloropicrin bringing together a dispersion in a water comprising medium of a chlorine yielding material and dispersions in a water comprising medium of picric acid and of lime.

6. In a process of making chloropicrin, bringing together a suspension in a water comprising medium of a chlorine yielding material and suspensions in a water comprising medium of picric acid and of an agent for neutralizing the dissolved portion of the picric acid.

7. In a process of making chloropicrin, bringing together a suspension in a water comprislng medium of a chlorine yielding material and suspensions in a water comprising medium of picric acid and of an alkali.

8. In a process of making chloropicrin, bringing together a suspension in a water comprising medium of a chlorine yielding material and suspensions in a water comprising medium of picric acid and of lime.

9. In a process of making chloropicrin, bringing together a dispersion in a water comprising medium of bleaching powder and a dispersion in a Water comprising medium of picric acid.

10. In a process of making chloropicrin, bringing together a dispersion in a water comprising medium of bleaching powder and dispersions in a water comprising me dium of picric acid and of an agent for neutralizing the dissolved portion of the picric acid.

11. In a process of making chloropicrin,

' bringing together a dispersion in a water comprising medium of bleaching powder and dispersions in a water comprising medium of picric acid and of an alkali.

12. In a process of making chloropicrin, bringing together under pressure a dispersion in a water comprising medium of a chlorine yielding material and dispersions in a water comprising medium of picric acid and of an agent for neutralizing the dissolved portion of the picric acid.

13. In a process of making chloropicrin, bringing together under pressure a dispersion in a water comprising medium of a chlorine yielding material and dispersions in a water comprising medium of picric acid and of lime.

11. In a process of making chloropicrin, bringing together under pressure a suspension in a water comprising medium of a chlorine yielding material and suspensions in a water comprising medium of picric acid and of an agent for neutralizing the dissolved portion of the picric acid.

15. In a process of making chloropicrin, bringing together under pressure a suspension in a water comprising medium of a chlorine yielding material and suspensions in a water comprising medium of picric acid and of lime.

16. In a process of making chloropicrin, bringing together under pressure a dispersion in a water comprising medium of bleaching powder and a dispersion in a water comprising medium of picric acid.

17. In a process of making chloropicrin, bringing together under pressure a dispersion in a water comprising medium of bleaching powder and dispersions in a water comprising medium of picric acid and of an agent for neutralizing the dissolved portion of picric acid.

18. In a process of making chloropicrin, ln'iuging together under pressure a suspension in a water comprising medium of bleaching powder and a suspension in a water comprising medium of picric acid.

19. In a process of making chloropicrin, bringing together under pressure a suspension in a water comprising medium of bleaching powder and suspensions in a water comprising medium of picric acid and of lime.

20. In a process of making chloropicrin, bringing together a dispersion in a water comprising medium of a chlorine yielding material and dispersions in a water comprising medium of picric acid and of an agent for neutralizing the dissolved portion of the picric acid, and subjecting the resulting mixture to steam distillation.

21. In a process of making chloropicrin, bringing together a suspension in a water comprising medium of a chlorine yielding material and suspensions in a water comprising medium of picric acid and of an agent for neutralizing the dissolved portion 260. CHEMISTRY, CARBON j CMPOUNDS.

of the picric acid, and subjecting the resulting mixture to steam distillation.

22. A process comprising bringing together a dispersion in a Water comprising medium of a halogen yielding material and dispersions in a water comprising medium of picric acid and of an agent for neutralizing the dissolved portion of the picric acid.

23. A process comprising bringing to- 10 gether a dispersion in a Water comprising medium of a halogen yielding material and dispersions in a Water comprising medium of picric acid and of an alkali.

24. A process comprising bringing together under pressure a suspension in a Water comprising medium of a halogen yielding material and suspensions in a Water comprising medium of picric acid and of lime.

ORLAND R. SWEENEY. 

